L.2. EuroEA3O24-IRMS Thecomplete instrument is shownonthephotograph below: It is of a compactdesign,occupying the minimumof laboratory space.It enjoys complete andeasyaccessibility to allitsinternal components andpafts,Top,rearand panels side areremovable, the entirefrontof the instrument consists of a moulded pafts, door,givingunhindered access to the internal Thesolidsample AutoSampler is located on the top panelof the instrument andis foreasyloading designed of samples.
Autosampler
BasicUnit
Keypad
EuroEA3024-IRMS
-B-
sub-units L.z.L. EuroEA3024-IRMS dividedinto the variousareasshownin the The EA3024can be conceptually photographs in thissection: The keypadis locatedat the front of Whenthe instrument is the instrument. immediately switchedON it becomes active. in Section 4 of is described Thekeypad alsocontains Thesection thismanual. required for using all the information thekeypad. Keypad by opening The GCovenis accessed instrument. It the front door of the enclosure consists of a well insulated which housesthe GC column,the Detector(TCD) ThermalConductivity together with a heater and a sensorfor temperature temperature regulation. in section The GC oven is described procedure for 2.5, togetherwith the GCcolumn. mounting GCOven
Front Furnace
(P/N EA201200) Front view removing Instrument front panel
at the righthandsideof the compaftment is housedin a wellventilated TheFurnace panel the isolation by removing shouldnot be accessed GCoven.Thiscompartment that causesthe electrical by a safetyinterlock on the front:the panelis protected OFFif thepanelis removed. to beswitched supplyto thefurnaces
Furnaces compartment Right'handview after removing Instrument lateral panel
-9-
pipecaneasilybe removedand replaced if needed,full and connecting The supports the sidepanelat the lowerpaftof the righthandsideof is gainedby removing access the instrument.
Electronics
Electronics
The Electronics are housedin two cabinets at the rearof the instrument and can be accessedby removingboth back panels.The Electronics are brieflydescribedi n section1.6.6.
GasControlAssembly
(EPCP/N EA20I222)and FiveON/OFFValves,three Electronic Pressure Controllers (P/N FlowMeter EA201224) one Electronic are mountedon a largeSS bracket,just abovethe GCoven.The valvesare all electrically operatedand are "NormallyClosed" (NC). Thevalvesare identified1 to 5 withtagsfastened to the respective electrical cables. Information andthe gaspathway canbe foundin section1.6.8 aboutthe pneumatics
-10-
1.2.5.
The GCoven
Insulated housing
SS nut (P/N EA20s01o)
GCColumn TCDHousing (P/N EA20L22O) TCDElectrical connections
whichcontains a bandheateraround housing of wellinsulated TheGCovenconsists Thetemperature insidethe ovenis the GCcolumn. enclosure containing the circular control temperature of the GC is regulated by a and by a thermocouple monitored (P/EA201242). cabinet in theelectronics Ovenlocated 6mm,length0,7mfor (NC). Steel,OuterDiameter isStainless TheGCColumn Protocol). columnis used(seeAnalytical For(S)a different Thesamplegasesflow resistors. typewith matched TheTCDis of a highsensitivity throughthe samplecellcarriedby Heliumcarriergas.The secondcellactsas a then flowsthroughthiscell,thisHelium flowof cleanHelium cell,a constant reference purposes, purging to as the it is referred for sample flowsinto the AutoSampler "Purge" Helium,
-13-
L .2.6.
The Gas Pathway
The instrument requires HeliumandOxygen. Thesegasesare admittedin the rearof the instrumentat the connectorsmarkedHe and 02 using IlB" gas fitting (P/N (Seepag.21) for IlB" tubing(P/NEA2060L2-2,5). EA3120) The Oxygengasis suppliedfromgascylinderto Oxygen"IN" Bulkhead (P/N Swagelok gas reaching EA3120) EPCafter flowingthrough"Oxygen filter" (P/N EA201235) passesthrougha restrictorand is isolatedfrom the restof the pathwayby two valves EV-2and EV-3.Two valvesin seriesare included labelled at this pointto guardfrom the potentialleakageof Oxygeninto the Heliumstream,in the eventof poorsealing by oneof the valves. manually Thevalvescanbe operated andindividually fromthe instrument keypad. Duringa RUNcycle,they open simultaneously at the start of the Oxygeninjection subroutine, they closesimultaneously whenthe requested volumeof Oxygen(set at the keypad)has beendispensed. Oxygenis normallyinjectedat a pressurein excess (setat the keypad)of the Heliumpressure, process. for a moreefficientcombustion to ON/OFF valveEV-1.It divides Heliumgasis supplied at the rearof the instrument, gaslineandthe Purgegasline. pathways, intotwo separate the Carrier -14-
gaslinethe Heliumpressure In the Carrier is set by the CarrierEPC-1 (Setat the keypad), flowis measured bythe Electronic FlowMeter(FM),thisreading its resulting canbe visualised Helium on the keypaddisplay. thenflowspastthe Oxygen admit pointandthrough the connector C-2at thetopof the instrument labelled "Carrier", It flowsthroughtheAutoSampler intothe Combustion bodyanddirectly reactorin the pipeand into the front furnace.At the bottom,it flowsthroughthe connecting reactorin the RearFurnace. viaa connector Reduction It re-enters the instrument C-4 locatedon the top panelof the instrument andflowsto the traps(if anyare in use) thenthroughthe GCColumn, the Carrier cellof the TCD,throughan ON/OFF valve panel EV-4andfinallyout of the VentportC-1located on the top of the instrument. At thispointa Ventfrit if mounted. pressure In the Purgeline, Heliumflowsinto an electronic controller EPC-2, the pressure required for thisHeliumis setat the keypadon the frontof the instrument. Helium flowsthrougha restrictor andthenthrough the reference cellof theTCD. valvelabelled It thenpasses throughthe ON/OFF EV-5,out at connector C-3located "Purge". andlabelled onthetoppanelof theinstrument It thenflowsintotheAutoSampler bodyat thebottomfaceof the Purgechamber, and ventsoutat thesample tray,just beneath theclearsample traycover.
9 pins Connector
Rear Oven
-15-
hasbeenincurreda detailedreport In caseanyexternaldamageto the instrument purposes. shouldbeprepared for insurance assoonas possible, to theinstrument, Thegassupply should beasnearaspossible
WARNING DONOTlift the EuroEA3O24-IRMS by the front door. Two peopleare neededto lift and carrythe instrument. Theyshoulddo so by holdingthe two beltsaroundthe instrument. ImportantSafetyNotice.
in the environment be dispersed and mustbe disposed of, in linewith local lawsandregulations.
2.5. Makingelectricalconnections 2.5.1. Electricalconnections Theinstrument is connected to theMainsPowerSupplyusingthe cableprovided with the instrument. on the rearpanelat the top left hand The Mainspowersupplyswitchis positioned fromthe frontof the instrument by usingthe right cornerand is easilyaccessible hand. pott. to he RS232 ThePCis connected connector. to thePCviaRS232 is used"OnLine",it is connected If a balance connections Seepage20 for RearPanelelectrical
2,6. Mountingthe GCcolumn mustbe mountedin the GCoven.To do that: A columnsuitablefor the application -23-
below45 oC. provided.
the GCoven'when bothconnections havebeensecured tighfly,the columnis thenre-positioned insidetheGCoven. If a columnis alreadyin placeand has to be removed, ensurethat the gas pathwayhas beendepresiurisedbeforehand. Thephotograph berowshowsthecorumn mounted in theoven: Columnconnectors Pull the sample and referencecapillaries out of the oven, then mount the columnusingthe reducing unions supplied.Use the Aluminium ferrulessupplied. Tightenquite hard on the connectors to obtaina qas tightseal. When the column is securelymounted,push it back into the oven and closethe ovendoor.
It may be necessary to conditionthe column,beforeusing.The conditioning procedure is reported in thesection 1.3of thismanuai.
-24-
2.7. Mountingreactors Theprocedure for mounting reactors isthesamefor bothfrontandrear reactors, the components involved areverysimilarwithdifferences whichdo not impinge on the procedure. Please ensurethat you usethe correctcomponents, i.e. front reactor holder whenmounting a frontreactor etc.... 2.7.L.
Mountinga reactorinto a reactorholder Reactortube (P/N Ef2509) "O" ring (P/N EA213535)
Holderretaining nut
ReactorHolder
Threadthe "O" ring overthe top part of the reactortube. Engagethe reactor into the reactor holder,to the very bottomof the holder Threadthe holderretainingnut overthe reactortube from the bottomend of the reactor.
untilthe reactoris securelyheld in the holder. Please note that: If the reactor is not firmly held in its holder, it may become detached during removal from the furnace.
-25-
2.7.2. Mountinga reactorinto the furnace
Warning THEFURNACEMUSTBESWITCHEDOFFAND COOLEDTO A TEMPERATURE BELOW45oC,beforeattemptingany of the stepsin this section. Failureto complymay resultin personalinjury! You are also strongly advisedto depressurisethe entire gas pathway, beforeremovingthe AutoSampler.
please, needed, followtheinstructions in section 3. procedure described in section 2.7
Youcanachieve thiseitherby turningthe supplyof HeliumOFFat the gas cylinderor by closingvalveEV1,whilstretaining valveEV4open.The gas pathway is described in section1.2.5andthe access to valveactions in section 4.5.3.
Thisis bestdonefromMethod 0, butit canoff coursebe donefromanyof the othermethods. Method0 is programmed duringtestat EuroVector. It is calledfromthe Menu keyMErl Thefurnaceparameter shouldbe setto OFF,Please, checkthat it is stillthe for thepurpose casebeforeusingthismethod of changing the Reactor. If unsure,pleasereferto Section4, whereall keypadoperations are fully described. Wait until the furnacehas cooledto a temperaturebelow 45oC,thenfollow the procedure described overleaf.
-26-
Slidethe entireassembly obtained fromthe previous section,intothe furnace,ensuring thatthe flatsof the bayonet lockareparallel to the flatsof the holein the Stainless Steel plate locatedon the top panel of the instrument. Ensurethat the reactor is not in any contactwith the furnacewall. (P/N EA20304O-B RearReactorHolder) (P/N EA203034Front ReactorHolder)
Pushthe assembly as far as it can go, checking first that the bottomend of the furnacehaslocatedcorrectlyintothe bottom "Quick-Fit" connector. Plugthe reactorinto the quick-fitconnector (thisrequires a smallamountof downward ring) forceto passthe sealing to Turn the entireassembly anticlockwise lockin position withthe bayonet lock
Thenewreactoris nowin place. cannowberemounted. theAutoSampler If it is a frontreactor, PTFE theconnecting tubingcannowbeputbackin place. If it is a rearreactor,
-27-
2.8. Removinga Reactor
WARNING MUSTBESWITCHEDOFFAND COOLEDTO A TEMPEMTURE THE FURNACE BELOW45oC,beforeattemptingany of the stepsin this section, Failureto complymay resultin personalinjury! You are also strongly advisedto depressurisethe entire gas pathwdyr beforeremovingthe AutoSampler.
Thisis bestdonefrom Method0, but it canoff coursebe donefrom any of the othermethods. It is calledfrom the Menu duringtest at EuroVector. Metpd_0is programmed
keyMrrl
The furnaceparametershouldbe set to OFF,Please,checkthat it is still the the Reactor, casebeforeusingthis methodfor the purposeof changing If unsure,pleaserefer to Section4, where all keypadoperationsare fully described. Wait until the furnace has cooledto below 45oC
You can achievethis either by turningthe supplyof HeliumOFFat the gas rylinderor by closingvalve EVl, whilst retainingvalve EV4 open.The gas pathwayis described in sectionL.2.7andthe accessto valveactionsin section 4.5.3.
-28-
the reactorholder,by turningthe Unlock holderclockwise to the"unlock"position.
Pull the entire Reactor holder/Reactor assembly upwards,until it has completely comeout of the instrument. Youareadvised to leverwith bothhandson the top of the instrument to gentlyextractthe reactor from its "QuickFit"connector at the bottom.This will ensurea smoother controlduringthe extraction of the reactor. the reactorin a safeplace.
2.9, Mountingthe AutoSampler pleasereferto section3 of this An entiresectionis devotedto the AutoSampler, and its operation together description of the AutoSampler manualfor the complete trouble mounting, and shooting. for dismounting withthefullsetof instructions
-29-
3.3. Installation
1 2 3 4 5 6 7 8
9 10 11 L2 13 74 15
body AutoSampler Sampletray assembly Sampletraycover Purgecapillary Carriercapillary Knurlednut mountingpillar AutoSampler Frontholdermountingconnector
Motorpowercable Motorpowersocket Purgegasconnector Carriergasconnector suppottbracket AutoSampler AutoSampler retainingscrew connector O-ringfor AutoSampler
(B) of . Bringthe AutoSampler pillar(7) abovethe mounting connector mounting the frontreactorholder. . Inseftthe connector thetwoconnectors' O-ring(15)between . Tightenthe knurled (6) nut securely. (13)to the top panelof the instrument suppoftbracket the AutoSampler Secure ' (14). screw usingthe largeretaining
-31 -
1 2 3 4
5 6 7
AutoSampler body Purgecapillary Carriercapillary Motorpowercable
Motorpowersocket Purgegasconnector Carriergasconnector
r Connect "Purge"at the backof (2) between the poft labelled the Purgecapillary "Purge"located on the top panel the AutoSampler body(1) andthe poftlabelled (6). of theinstrument . Connect "Carrier" (3) between at the backof the poftlabelled capillary the Carrier port thetop panel located on labelled "Carrier" body(1) andthe theAutoSampler (7). of theinstrument . Connect "Cap" the motorpowercable(4) to the motorpowersocket(5) labelled panel of theinstrument. on thetop -32-
Caution Takecarewhen you mount the Purgeand Carriercapillaries,that you engagethe connectorsin goodalignmentwith the connectorthreads in the AutoSamplerbody and that you screwthem in gentlv without crossthreading. If the threadsbecomedamaged,the entireAutoSamplermay haveto be replaced.
'
. Slidethe sample (1) and(2) overthe sampletray upperactuation trayassembly slot(3)foundon the underside of thesample block(7) suchthatthetray locating pin(4)foundon the sample trayupperactuation tray(2) slides overthe locating (7). block . Rotatethe sampletray assembly pin (5) foundon CLOCKWISE untilpositioning groove is insidethe positioning top andat the frontof the AutoSampler assembly (6) foundat the sideof the sample trayplate(2).Thismaintains the sample tray position, platein onlythesample trayto advance duringoperation. allowing
1 2 3 4
1" sampletray Sampletray plate Traylocatingslot Tray locatingpin
5 6 7 8
pin Positioning groove Positioning Upperactuationblock Sampletray cover
. If thesecond thenaddit abovethefirsttray. is required, trayprovided sample . Placethe sampletraycover(B)overthe sampletray assembly. Duringanalysis, purging of thesamples. for efficient thiscoveris essential -33-
3.4. Troubleshooting Observedfault
Suggested causes
Action
Thepistonis not movingin andout,
TheAutoSampler is unplugged.
Connect the powerplugat the top faceof the instrument.
TheAutoSampler is disabled at the keypador the software,
Re-enable the AutoSampler eitherat the keypad(Appendix B) or fromthe software inteface.
Thesampletrayassembly has beeninstalledcorrectly.
Checkinstallation of sampletrayassembly (referto sectionentitled"Installation,). if the faultpersists,pleasereferto Appendix 7.
Thesampletray doesnotseemto advance correctly.
The sampletray actuationblockhas not been installedcorrectly,
Checkinstallation of sampletrayactuator (Referto Appendix 5). Thesamplertray coveris not in place. Placethe sampletray coveroverthe sampletrayassembly.
Thereis a large blankduringthe AutoSampler test (TheAutoSampler A samplehasnotdropped or thereis Thepistonmustbe cleaned.Referto test is described on samplematerial in the pistonchamber. Appendices 4 and5 for removing and the instrument remounting the piston. installation procedure). Thepurgeflowis toosmall. Usinga flow metre,measurethe purgeflow out of the instrument at the "purge,, connector. If youcannotobtaina flowof B0ml/min, contactyourlocaldistributor.
Thepistondoes completeits full travel,
Thereis a leakat oneof the pistonOrings.
Checkfor evidence of a leak.(Referto Appendix 3).
Thetray actuationblockhasnot been mountedcorrectly.
Referto Appendices 4 and5 to inspectthe positionof the tray actuationblock,
Thereis a mechanical obstruction in the pistonmovement,
Thepistonmustbe takenout and inspected so the obstruction canbe eliminated. (Refer to Appendices 4 and5).
Thereis a problemrelatedto the motor.
Contactyourlocaldistributor,
Thesampledoesnot Thesampleis too big,it is probably jammedat the top of the sample drop injector. It is not possible to At somestage,materialfromthe viewinsidethe reactorhasbeenthrownup to the reactorthroughthe quartzwindowandditied its lower viewingmirror suface.
-34-
Remove the sampletrayassembly and removethe samplefromthe sample injectorusinga pairof tweezers. Removethe reactorandcheckthat the plug of quaftzwoolis not in theAutoSampler. Clean, Thequartzwindowmayneedcleaning. To accessthe window,pleasereferto Appendix 1, whichgivesan exploded view of the completeAutoSampler.
Section4 KeypadOperation 4.L. Descriptionof the keypad The instrument canbe fullyoperated fromthe built-inkeypadlocatedon the front panelof the instrument. Thekeypad is shownonthe photograph below:
Arrow keys
Kevoad disolav
Thekeypadbecomes activewhentheinstrument is switched ON. It contains 3 setsof pushbuttons:
lMEtrandffi FrARl,ffi anolrlrrE The displayon the keypadincludestwo lines:The top line indicatesthe namesof parameters and submenusincludedwithinthe pafticularmenu.Directlybeloweach parameternameon the secondline,the valuefor the particular parameter is shown.
-51 -
4.2. The set of 4 arrow keys 0 O 3 C The horizontal movement arrows3 G enablehorizontal of a blinking cursor,The parameter selection of a pafticular or submenu is madeby placing the cursoron the parameter required andmaking it blink. The up anddownarrows0 O act on the parameter valuewhichis blinkingand of its value.Allowed valuesare foundby scrolling allowsmodification with these the listsprovided, arrowsthrough In general, the useof the arrowkeysis as outlined above,however therearea few exceptions to the simplerulesdescribed aboveandthesewill be described whenever theyoccur.
4,3. The HOMEmenu Whenthe instrumentis flrst switchedON,a displayappearsgivinginformation on the instrurnent configuration andthe firmwareversioncurrentlyinstalled. In the caseof the EuroEA-3024or 3028 models,this displayshows:EuroEA3000 seriestogetherwiththe firmware versionissuenumber, After 5 seconds,this displayautomatically disappears and is replacedby the HOME to re-access the statusinformation, display.I!!-lg necessary thenthis canbe doneby pressing the HOMEdisplay. lEXITifrom The HOMEmenu,is a set of 4 displays, showingthe currentvaluesof a numberof parameters. Fromthesedisplays,information can be read,but cannotbe changed, given,resultsfromthe internalmonitoring The information of the shownparameters, parameters if these change,thenit is possible to visualise the changesas theyoccur. An example is the changein the Frontoventemperature, duringthe warm-upperiod, In orderto visualisethe full set of parameters, it is necessary to use the horizontal arrowkeys3 C, causingthe parameters to scrollacrossthe screen.
-52-
menuaredescribed below: Theentries ontheHOME STS
is a recordof thecurrentstateof theinstrument. it displays willbeoneof thefollowing states: Theinformation STD-BY
state if the instrument hasbeenputin a Stand-By
If the instrument eitherto reachsetvalues is conditioning COND (forexample, warmingup)or to allowpressure to stabilise aftera valve action. READY Whenall the operating conditions for the currently loaded method arefulfilled thenREADY appears. Whenthe instrument is performing RUN a run cycle,then RUN appears, It is possible to haltmomentarily a run cycleby pressing HOLD The cycleis put on holdand the the commandpushbuttonlSTOPl. on HOLDuntil the operatoreither displayshowsHOLD.It remains presses the command button|STARTIto continue the analysis, or presses to abodtheanalysis cycle. thecommand buttonSTOP Whenthe solidAutoSampler is not fittedor is disabled, SPEC (Special) thenSPEC appears. If a fault appears,then the nature of the fault is ALARM is repoftedin the immediately flagged.The full list of alarmmessages at the endof thismanual. appendix TO ACCESSOTHER rF A FAULTrS FLAGGED,rT rS POSSTBLE VALUES. DISPLAYSAND CHANGEPARAMETER to a more Thisfacilityenablesthe operatorto modifyceftainconditions pafticular fault repofted. in view of the state desirable repoftsthat a largeleakhasoccurred. Oneexample:The alarmmessage possible to accessthe displayswhichwill enablethe operator Thenit is to switchoff the Heliumadmitvalve,stop an on-goingrun, switchOFF the TCDetc....
-53-
MTH TIME
here' is displayed loaded currently of themethod Thenumber sincethe elapsed thenthetime(inseconds) If a runcycleis in progress, of theruncycleis shownhere' beginning --thena shortdottedlineis displayed If a runcycleis notin progress,
here. FLOWCARRIERThecurrentflow(in mlimin)forthecarriergasis displayed PURGE
is the solidAutoSampler Thecurrentflow(in mymin)of Heliumpurging here' disPlaYed
gasis indicated (in kPa)of the carrier Thecurrentbackpressure CARRTER PRESS here. oz AP
(in kPa)in excessof that the oxygenpressure displays Thisparameter is shownby the gaspressure TheCarrier gas'pressure. of the Carrier previous entry.
here' is displayed (in "C)of thefrontfurnace T:FRONT Thecurrenttemperature REAR
here is displayed (in "c) of therearfurnace Thecurrenttemperature
OVEN
here' (in"C)of theGCovenis displayed Thecurrenttemperature
-54-
4,4, The STOP, START, EXIT and ENTERCommand keys
Frof,
fromwhichthe runcyclecanbereStopsa runcycleputtingit on,HOLD, theISTAR'I button.Whenpressed a second staftedby pressing time,the returns runcycleis aboftedandthedisplay to the 'Home'display. Pressing the ISTART buttoninitiates an actionwhichhasbeenselected fromoneof the menus: It staftsthe Runcycle(Analysis) if the displayis set for runninga sampleand the statuson the 'Home'displayshowsthat the instrument is Reap]y=_Qg,ware that if the instrument is not 'Ready', thenpressing theISTARTI buttonwillnot resultin anyaction.Therun cycledoesnot startandwillnotstaftuntilthe instrument statesthat it is 'Ready' It staftsa leaktestif theleaktestsubmenu hasbeenselected. This commandkey resultsin differentactionsdependingon the menu fromwhichit is pressed:
effect.
callsthe 4th MFf menuwith tle 'STO'option blinking,invitingthe commandbutton for saving the operatorto press the IENTERI pafticular parameters method. enteredin this displayto the 'Home'displa/-{hen a submenufrom the SP-Fmenu the IEXITI buttonreturnsthe displayup by one is active,then pressing menu. levelto the ISP-E
-55-
key resultsin differentactionsdepending Thiscommand on the menu fromwhichit is pressed: parameters entelgdin the pafticular method.Please notethatsaving can 4* only be done from the by pressing lrNrrRl lwil menuand is blinking. onlywhenthe'STO'option of oneof the4 functions the selection available: STBY, CLOCK, CNTS special function Thedesired mustbeselected firstusingthe or TEST. keys3 G, untilitsnameis rnadeto blink. horizontal 4.5. The SET, MET and SPC-FPush Buttons theconfiguration menuforthe instrument. TheI SETI buttonaccesses parameters the menuconcerning all the analytical The IMFT--I buttonaccesses for parameters All the method arecontained withina setof 4 different sampleanalysis. eachoneselectable by usingthehorizontal arrowbuttons3G displays, to a menuof special functions whichwillbedescribed fne I SpC-Flgivesaccess later in thissection. Whenthe operatorselectsone of the menusindicated aboveby pressingthe button,the buttonlightsupconfirming theaccess corresponding to the menu. menu,the lit buttonfor thatparticular menuneedsto In orderto exitfroma selected The lighton the buttonthendisappears; access to that menuis thus be pressed. terminated havebeenmadeto anyof the entriesin the lsffl menu,thenthese If anychanges saveduponexitingthe menuby pressing on its push changes are automatically button. then,changes However if the Mfr rgnu hasbeenselected, arenotsavedby simple of thelMFfI menu. de-selection made, then: In orderto saveanychanges il*n pressENTER STOblinking), to blink,thenpressIENTERI -56-
CAP 4.5.1, TheSETmenu:MODE,METHOD, to a numberof itemswhichneedto be declared, TheFfr menukeygivesaccess mostof theseitemswill alreadyhavebeenset at is operated, beforethe instrument thetimeof testingby EuroVector. anyof theseitems,presstheE button.Thisactioncauses In orderto setor change ThefullISET menuis displayed. the buttonto lightupanda 'Blip'canbeheard. a second time,the In orderto exitfromthismenu,theFd buftonmustbe pressed returnto theHOME menu, lightonthebuttonswitches off andthedisplay as soonas they are made. All modifications are savedautomatically it is deactivated automatically If the 15fr menuis not usedfor 10 seconds, andthe menu. returns to theHOME display automatically MODE
The instrument can be controlled eitherfrom its own built-inkeypad (LOCAL) or from the PC(PC).The modeof controlhasto be declared underthissubmenu. cursorto MODE. To settheControlmode,bringtheblinking is controlled viaa PC,thenPCis selected Whenthe instrument by using the'upanddown'arrowkeys0 o. viathe keypad, is controlled thenLOCAL is selected Whenthe instrument keys0 o. byusingthe'upanddown'arrow
MTH
to pre-program fromthe key It is possible andstoreup to 10 methods, pad.A pafticular fromthissubmenu. methodis selected method,bringthe blinkingcursoroverMETHOD To selecta pafticular andusethe 'up anddown'arrowkeys0 o to scrollthroughthe listof is found, method methods, untilthe required
CAP
and must be set to YESas the This refersto the solidAutoSampler, is fittedwith a solidAutoSampler. instrument bringthe is fittedto the instrument, To declarethat a solidAutoSampler blinkingcursorto CAPand use the 'up and down'arrow keys 0 O to selectYES. -57 -
and allowsperforminga run SelectingNO disablesthe AutoSampler a samPle, withoutinjecting TCD
the TCDONandOFF. allowsswitching Thisparameter parameter, horizontal arrowkeys3G to makeit the use To selectthis blink,thenusethe 'upanddown'arrowkeys0 O to selecteitherONor OFF. are Whenthe TCDis switchedON,accessto the TCDsignalparameters
bypressing accessed mTEn
ZERO Setsthe levelfor the zero balanceof the TCD bridgei.e. SET the levelfor the outputbaseline. Readsthe signal(in mV)acrossthe TCDbridge. LEVEL POLARFY Setsthe polarityfor the TCDsignal. Setsthe gain GAIN
4.5.2. TheIMEImenu are Thevariousparameters andsaveup to 10 methods. to pre-program It is possible setfromtheMFI menu. If you have made changesto a method,and then decidethat you do not wish to keep these changes,but wish to return to the original parameters the savingprocedure.Oncechanges stored,this MUSTbe done BEFORE havebeenmadeand saved,then all the originalparametersof the method are irretrievablylost, In order to return to the original parameters,push the EXII command buttoryto accessthe 5thME! menu,ensurethat STOis blinking,then push the leXflcommandbuttona secondtime. you are strongly or usingthe keypad, If you are unsureaboutmakingchanges storedwithina method,before to makea noteof the originalparameters advised to makeanychange. attempting pressthe|ME b$q. Thisactioncauses the methodparameters, In orderto access canbe heard.ThefirstMffl menuis displayed. the buttonto lightup anda 'Bleep' Thereare5 menusin total -58-
a set of 2 vefticalarrowkeys On the extremeleft handsideof eachmenudisplay, O. O down' arrow keys 0 whenthisis blinking, the 'upand appears Pressing enables to the nextmenudisplay. to movefromonemenudisplay Menudisplays: Thefirst IMETI MTH
number Thisentryshowsthe method currently loaded. cursorto MTHandusethe 'up anddown'arrowkeys Bringthe blinking 0 o to selectthe required methodnumber. Oneof 10 methods labelled fromtheallowed list. from0 to 9 canbechosen
CAR,KPa
Thecarriergaspressure in kPais setwiththisparameter. Bringthe blinkingcursorto CARRIER andusethe 'up anddown'arrow keys0 O to selectthe requiredoperatingpressure. The list allows pressures in the rangeof 10to 200kPain stepsof 1 kPa.
Pur.mLm The Flowof Helium(in ml/min)purgingthe sampleis set with this parameter. Thesampleis purgedwith Helium,priorto beingreleased intothe reactor. Thisflowis allowed to takevaluesbetween 10 and200ml/minandcan in stepsof 10ml/min. be incremented Bringthe blinking cursorto thisparameter andusethe 'up anddown' purgeflow. arrowkeys0 O to selecttherequired ThesecondimEIMenudisplays: OzVol
allowsselection This parameter of the volumeof Oxygen(in ml) which the sample. will be injectedfor combusting Bringthe blinkingcursorto this parameter and use the 'up and down' arrowkeys0 O to selectthe requiredvolume.The list allowsvolumesin the rangeof 1 to 200 ml in stepsof 1 ml. The OFFfacilityallowsperformingruns, without the injectionof any Oxygen.
oz AP
This parameterallowsselectionof pressure(in kPa)at which Oxygen the pressurein whichwill be injectedinto the reactor.This represents excessof that of the Heliumcarriergas.
-59-
andusethe 'up anddown' cursorto thisparameter Bringthe blinking The list allows arrow keys 0 O to selectthe requiredAPressure. in therangeof 15to 300kPain stepsof 1 kPa, APressures
TIME
purpose andis shownfor information Thisentrycannotbechanged only. (in seconds) injection. of the Oxygen Thisis It represents the duration volume selected. andpressure ontheOxygen dependant TIME volumehasbeensetto OFF,thenthe entrybeneath If the Oxygen alsoshowsOFF.
Menudisplays: Thethird IMETI SMP
Thisparameter setsthe Sample delaytime(in seconds). Bringthe blinkingcursorto SMPand usethe 'up and down'arrowkeys sampledelaytimeThe listallowstimesin the 0 O to selectthe required in stepsof 1 second. rangeof 0 to 99 seconds
RUN
with this parameter. is selected The samplerun time(in seconds) Bringthe blinkingcursorto RUNand usethe 'up and down'arrowkeys 0 O to selectthe requiredsamplerun time The list allowstimesin the in stepsof 1 second. rangeof 10 to 999 seconds and the When the instrumentis used with a mass spectrometer, AutoRunsequenceis set and controlledfrom the massspectrometer datasystem,then the RUNtime mustbe set to a value which is less time on the mass than that declaredfor the singlerun data acquisition datasystem. spectrometer Analyseris READYby the time the This is to ensurethat the Elemental for datasystemstartsthe singlerun dataacquisition massspectrometer the nextsample.
-60-
Thefourth lMEi Menudisplays: FRONT
for thefrontfurnace allowsselection of thetemperature Thisparameters cursorto FRONT and usethe 'up anddown'arrow Bringthe blinking frontfurnace temperature keys0 O to selectthe required in the rangeof 500 to 1100"C for the The list allowstemperatures EuroEA3024-IRMS and in the range of 500 to 1300 oC for the stepis 1oC. theincremental EuroEA302B. In bothcases furnace OFF. TheOFFstatusallowsswitching theFront
REAR
for the rearfurnace Thisparameters allowsselection of thetemperature cursorto REAR andusethe 'upanddown'arrowkeys Bringthe blinking temperature rearfurnace 0 O to selectthe required in the rangeof 500to 1100oC,in stepsof Thelistallowstemperatures 10c. theRearfurnace OFF. TheOFFstatusallowsswitching
OVEN
for theGCoven. of thetemperature Thisparameters allowsselection cursorto OVEN andusethe 'upanddown'arrowkeys Bringthe blinking frontGCOventemperature 0 O to selectthe required in the rangeof 40 to 190oC,in stepsof The listallowstemperatures withtheOFFstatusfor switching the ovenOFF. loC,together
Menudisplays: Thefifth IMETI hastwo utilities: METHOD SAVING
(i) to copy the entire methodto a different methodnumberand to thenewmethodnumber. savetheparameters Theactualmethodnumberis shownby the firstnumberon the left handsideof thedisplay. cursorto the secondmethodnumberon the right Bringthe blinking the arrow + andusethe 'up anddown'arrowkeysto handsideof selectthe new methodnumberyou wish to use for savingthe parameters. Then,take the blinkingcursorto STOand pressthe command thatthe buttonlfruffnl Twoshottbleepscanbe heard,confirming actionhasbeenregistered' saving
-61 -
Nowthatsavinghasbeenperformed, it is possib@ menuby pressing on the lmffl menupushbutton.Thelighton tf'e buttonswitches off. notethatin orderto escape Please fromthelMFlmenu,i.e.'switch off the lighton thisbutton,tlqflle operator musteitherSavethe changes by pressing on the IENTERI command buttonwhenSTOis escape without saving any blinking or of thechanges, by pressing on whenSTOis blinking. thelEXITicommand button
(ii) To savethe method parametersin the actual current method The actualmethodnumberis shownby the first numberon the left handsideof the display. Bringthe blinkingcursorto the secondmethodnumberon the right handsideof the arrow+ andensurethatthe samenumberasthat If it is different,then you must of the actualmethodis displayed. makethe 2 numbersidentical. Then, fake tfe blinkingcursorto STO and pressthe command Two shortbleepscan be heard,confirmingthat the buttonIENTERI, savingactionhasbeenregistered. Nowthat savinghas beenperformed,it is possibleto exit the |Md menupushbutton.The lighton the menuby pressing on the IMETI buttonswitchesoff. Pleasenotethat in orderto escapefrom the ltqEtrmenu,i.e. 'switch off the lighton this button,thenlhe operatormusteitherSavethe changesby pressingon the ENTEEcommandbuttonwhen STOis withoutsavinganyof the changes, blinking or escape by pressing on the IEXITI commandbuttonwhenSTOis blinking.
-62-
4.5.3.
CNTSand TEST TheSPC-F,SpecialFunctionsmenu:: STBY,CLOCK,
STBY
This submenuallowsthe operatorto selectone of the Stand-by by pressing configurations ENm whenthe STBYfunctionhas been (bring the blinkingcursorto STBY,by usingthe causedto blink subfunctions: arrow3 G keys).Thereare3 STBY horizontal selected usingthe 'up and down'arrows0 o. Theseoptionsare described below: switchedOFF.Energyis saved The TCDis automatically off,Thisallowstheoperator to perform andGasis switched of maintenance tasks which best conducted a number are withgascompletely turnedoff. switched OFF.Energy andGasis TheTCDis automatically is reducedto 70o/oof saved.The furnacetemperature temperature and Heliumflow is stopped,Every operating hour, heliumis admittedagain,to ensurea constant environment of helium. switchedOFF.Energyonly is The TCD is automatically is reducedto 70o/oof its saved,The furnacetemperature gasis stillflowing. value,butHelium operating conditions have Indicates that noneof the threestand-by This escaping from a selected. option allows Stand-By been state,
GASOFF
GASSAVE
ACTIVE NONE
possible On 'Wakeup' of the instrument. to requestan automatic stateandrewill get out of its Stand-by 'Wakeup' the instrument Therequired timefor gettingout itself,readyfor operation. condition READY submenu. SETUP' is enteredin the'AUTO of Stand-By facilityis requiredit is activatedby settingthe If the AUTOREADY parameter to ON(byusingthe'upanddown'arrows0 AUTOREADY
o ).
by setting facilityis not requiredit is de-activated If the AUTOREADY parameter to OFF(by usingthe 'up and down' the AUTOREADY arrows0 O).
-63-
Thedatein MonthandDay,as wellas the timeon the particular in thissubmenu, by selecting day,in HourandMinuteareentered (usethe horizontal arrowkeys3 G to sequentially theseparameters parameters in turn).Theactualselection selecteachoneof these of is doneby scrolling valuesfor theseparameters the appropriate up listsusingthe 'upanddown'arrowkeyso anddownthe available o. At the set time, the instrument will exit from its Stand-By itself conditions. to re-condition to fulloperation start conditions and CLOCK
to settheactualdateandtime. theoperator Thissubmenu enables for settingthe date and time, bringthe To accessthe parameters submenu, usingthe horizontal arrowkeys blinking cursorto the CLOCK thedateandtimeentrydata. to reveal 3 G, thepressENTEd yearswiththe'up year(Y)byscrolling thelistof allowed Entertheactual keys0 O. anddown'arrow (M),thenthe day(D), procedure for the monthinformation Repeat this (M) followed bytheHour(H)andminute
CNTS
theoperator to readthe statusof eachof a setof enables Thissubmenu A, B,C,D, E andF.andto resetanyof thecounters labelled 6 counters to0 by 1 eachtime the mR-i key is pressed Eachcounterincrements manually or a lStnx=isignalis sentfroma datasystem. The allocationof countersdescribedbelow must be taken as a In reality,any countercan be ratherthanan obligation. suggestion wishes. to anything thattheoperator allocated
allocation: Suggested
A B
c
D E F
FrontReactor RearReactor GCColumn Trap Spare sinceinstallation Totalnumber of analyses
-64-
the totalnumberof samples If counterF is usedto monitor analysed of the instrument, thenthis counter fromthe time of the installation be resetto 0. shouldNEVER relatingto the counters, bringthe blinking To accessthe information arrowkeysC C, then submenu, usingthehorizontal to the CNTS cursor
press lrrurrnl.
of a counter is readonthetopline, Thestatusnumber pafticular counter, To reseta bringthe blinkingcursorto the pafticular The arrowkeysI G and pressIENTERI. counterusingthe horizontal returns to 0. of countsimmediately number TEST
TESTfacilities: to 3 automatic Thismenugivesaccess manual. thistest,selectit with_!!g_[!nking cursorusing In orderto perform press arrowkeysc G and the horizontal IENTERI. shows: Thedisplay TEST: LEAKAGE PRESS TORUN START you ready to start the test, presstne lfrufenl As soon as are keyandthe LEAK testwillstaft. command will appearon the display, At the end of the test, a message whether the TEST hasPASSED or FAILED. theoperator informing arrowkeys3 G, selectCAPandpresslf nffnl : Usingthe horizontal IN
the pistonmovesinto the Whenthis actionis selected, AutoSampler bodyto the endof its travelandstopsin that position. whenremoving the pistonfromthe Thisposition is required seesection 6.2) AutoSampler body.(Please, It is usefulwhenleaktestingthe pistonsealingrings.(see section 3.5.7)
OUT
the pistonmovesout of the Whenthisactionis selected, AutoSampler body,to the endof its travelandstaysin that position. rings is usefulwhenLeaktestingthe sealing Thisposition (Please, 3.5,7) seesection onthepiston. -65-
AUTO
When this actionis selected,the AutoSampler completes piston entirecyclesautomatically. That is, the movesIN, then OUT and the Carouseladvancesby one sample position, The numberof cyclesshowson the display.This test is usefulwhen checkingthat the Carouseladvances correctly.It is possibleto correlatethe numberof cycles completed as shownon the displaywith the numberof This samplepositionsactuallyadvancedby the Carousel. the Indexer the sample Carousel. numbercanbe readon of (Please, seesection 3,6)
AutoSamplerDelay By pressingIENTERIfrom any of the entrieson the CAP to set a delaytime (in seconds) TESTmenu,it is possible piston the AutoSampler returnsto its OUT of beforethe position. Thedefaultvalueis setto 1 second,but it is possible to set it to anyvalueup to 30 seconds. Use the "up and down" arrow keys 0 O on the entry DELAYAFTERCAPIN to selecta delaytime from the list of allowedvalues. EV This test enablesthe operatorto manuallyactuatevalves fittedto the instrument. has5 valveslabelled1 to 5. The instrument line. Valve1 is fittedin the Heliumadmission Valves2 and3 are fittedin seriesand are usedfor isolatingOxygen from the Heliumcarrierstream,when closed,and for injecting whenbothvalvesare open. Oxygenintothe Reactor Ventline 4 is fitted in the Carrier Valve line,betweenthe TCDreference cell Valve5 is fittedin the reference purge inletat the solidAutoSampler. outletandthe Pleasereferto the diagramin section1.2.5whichshowsthe position of thesevalvesin the gaspathway. To open a pafticularvalve,use the horizontalarrow keys 3 G to to 1, selectit thenusethe 'upanddown'keysto setitsvalue(Status) To closea particularvalve,use the horizontalarrow keys C G to selectit thenusethe 'upanddown'keysto set itsvalue(Status)to 0.
-66-
5,3, Programming a method Whenthe instrument is testedat the EuroVector factory, methods areprogrammed as follows: Method0 offersHeliumflowthroughthe system,but the furnaceand ovenareswitched OFF.Theparameters are: MTH O (kPa) 6s CARRIER PUR.ml/min 80 ml/min OzVol 20 O zAP 35 SMP 6 RUN 32O FRONT OFF REAR OFF OVEN OFF METHOD O-+O Thismethodcanbe modified but it is stronglyadvisedto keepit as it is.It canbe veryusefulin a numberof situations, likechanging the reactor andperforming leak testingat roomtemperature. Up to 10 methods can be programmed andstored,the procedure for programming methods is described in Section 4,5.2. Actions thattakeplaceduringa "RUN"cyclearedescribed in the nextsection, these includeValveactionsand their timingsare programmed by the entriesto the parameters: SMPandRUN. Theparameters whichhaveaneffectontheoperating conditions are:
qualityandthe quali$of the canaffectthechromatographic ALLof theseparameters andIsotopic determinations, results, bothfor theElemental analytical for each sample type, need to be established conditions Optimum -7L-
5.5. Loadingand sealingsamplesin Tin Capsules. Theloadingandsealingof sampfes in nn capsules is impoftant for obtaining good analytical resultsandfor ensuring troublefreeoperation of the AutoSampter. Some recommendations aremadein thissection: sample, largecapsules forsamples uptg 40-50mg. Besureto selectthesizesuitable to yoursample size. Tn. lJu
maintained in absolutely cleancondition and that it is meticulously cleaned preparation beforethe of differentsampletypes.Cleaning is bestdoneby thorough wipingwitha softtissue. theycanbe usedstraight fromthecontainer supplied. Do Nor HANDLETHEcAPsuLEsBY HAND,always use clean tweezers. Standthe Tin capsulein oneof the holesof the capsulepreparation blockand loadthe required amountof sampleintoit, usingthe cleanspatulaprovided. Usingthe tool provided,squeeze the top of the capsuleto closeit. Movethe closedcapsuleontothe top of the block. Usinga set of tweezersin eachhand,gently and carefully fold the capsule severaltimes,in all directions so as to obtaina tightly packedand spherical "ball". Youmusttakegreatcarenot to damagethe tin foil with the tweezers, as this couldresultin the spillage of someof the sample. The resultingball shouldbe tightlypackedto ensurethat the sampleis well sealedinsidethe capsuleandevenlysurrounded by tin foil.Whenthe capsuleis droppedinto the hot reactor,it is importantthat the combustion occursin one single step, i.e. the tin capsulemustigniteat the sametime as the sample,to providethe highestheatof combustion to the sample. The finalgeometryshouldbe as spherical as possible to preventanyjamming insidethe AutoSampfer,
-78-